Multiphase continuous fat treating



' March 9, 1943. B. WINER MULTIPHASE CONTINUOUS FAT TREATING 2Sheets-Sheet 1 Filed Jan. 29, 1941 l m nglglgl,

INVENTO R. Barucfi W/n er" March 9, 1943.

B. WINER MULTIPHASE CONTINUOUS FAT TREATING Filed Jan. 29, 1941 2Sheets-Sheet 2 {my 127 mi INVENTQR; Earl/c6 Mner %mw. MW

Patented Mar. 9,

Baruch Winer, New York, N. Y.

Application January so, 1041, Serial No. 376,445

in Bumanla March 22, 1940 4 Claims.

I This invention relates to the hydrolysis or splitting of glycerides,as for example vegetable and animal oils and fats.

It is an object of the present invention to provide an improvedcontinuous counter-current method of effecting splitting or hydrolysis.

It is a further object of the invention to provide an improved processof hydrogenation and fat splitting.

In accordance with the method of the present invention, a body ofglyceride, as for example fat or oil, is passed upwardly in a columnagainst a downwardly flowing stream of water. Both the water andglyceride are maintained at a fat splitting temperature, the pressurebeing such a is necessary to maintain the water in a liquid conditionatthe desired temperature. During this process an emulsion is formedcontaining water, glycerine and a fat or oil component, and at each of aplurality of stations the emulsion is separated into a fatty or oilycomponent and a glycerine-water component, this separation beingeffected by passing the emulsion into contact with a porous filteringmedium. At the same time the upward passage of the glycerine-watercomponent is arrested and said component is caused to pass downwardlyand the fatty component is caused to pass upwardly. In this way aplurality of separate fat splitting zones are established andmaintained, these zones being separated by the emulsion separatingstation's.

By preventing the passage of the separated glycerine-water componentfrom a lower to an upper splitting zone, the concentration of glycerinein the water in the several zones is decreased and the fat splittingactivity of the water therein is increased.

In other words, at each separating station the emulsion is separatedinto its glycerine-water component and fatty component. Theglycerinewater component is returned to the immediately preceding orlower splitting zone and the fatty component is passed to the nextsucceeding or upper zone. Preferably the water is sprayed or finelydivided in its downward passage through the tower, and in order toproperly maintain this condition the water at each separating zone iscollected and re-sprayed into the next lower zone. Preferably, also, thefat or oil is sprayed into the tower at the bottom thereof and at eachseptional function of hydrogenation in the presence arating zone isre-sprayed upwardly. Thi may be accomplished by causing it to passthrough nozzles or orifices which impart a swirling movement to said oilor fat.

of hydrogen gas introduced into the column.

Furthermore, the glyceride, prior to its introduction into the column,may be partly or wholly hydrogenated by passing counter-currently to orconcurrently with a stream of hydrogen at a hydrogenation temperature inthe presence of a suitable hydrogenation catalyst, and then withoutcooling and without exposure to the air the still hot, hydrogenatedglyceride may be introduced into the fat or oil splitting column.

The principles of the invention will be described in the claims and willbe illustrated in the following detailed description taken in con-Junction with the accompanying drawings, in

which:

.Fig. 1 is a diagrammatic view showing the splitting column, means forheating the glyceride and the water and for cooling the fatty acidsunder controlled pressure;

Fig. 2 shows diagrammatically a column similar to that shown in Fig. 1in conjunction with a series of columns for effecting hydrogenation ofthe glyceride prior to its introduction into the glyceride splittingcolumn;

Fig. 3 shows a series of columns constructed similarly to the columnshown in Fig. 1 and intended for operation in series;

Fig. 4 is an enlarged diagrammatic view of a means for separating theemulsion at each of a plurality of stations and for re-mixing orspraying the water and glyceride at each of those stations;

Fig. 5 shows a series of columns for eifecting prehydrogenation bypassing glyceride and oil counter-currently as contrasted with theapparatus for concurrent flow illustrated in Fig. 2; and

Fig. 6 is a diagrammatic plan view of the enlarged view shown inelevation in Fig. 4.

Referring specifically to the several views in which like parts areindicated as far as possible by like numerals, and referring first toFig. 1, the column i is provided with an inlet 2 for hot In accordancewith that phase of the invention 56 w ter terminating in a spr y head 3and an let 6 for glyceride terminating in spray head I. At the bottom ofthe column there is an inlet I for hydrogen provided with valve II.There is also provided adjacent the bottom of the column I, a separatingvessel ll connected with the column I by pipes I and iii. .The vessel Itis equipped with draw-oil pipe I9 provided with valve I9. The vessel Itis further equipped with an inspection glass 20 and the column I isprovided with a similar glass 2i. From the top of the column, pipe 23provided with pressure gauge 24 and regulating valve 25 leads to heatexchanger 27. This comprises a series of tubes 30 connected at theirends to the tube sheets 8| and 82.- Pipe 84 leads from the bottom of theexchanger to tank 35 provided at the bottom with draw-0d pipe 36 havingvalve ill, and adjacent the top with pipe 38 and valve 39. The heatexchanger 21 also has water inlet pipe HI and water outlet pipe 42', thelatter leading to water tank 44. From the tank Mi pipe 85 leads to pump46, from which pipe ll leads to heating coil 48 connected to pipe 2which is the inlet pipe for water to the column i. The heat exchanger 21isfurther equipped with hydrogen eduction pipe 00 provided with pressuregauge 5i and valve 52.

From the oil storage tank 55 pipe 56 leads to pump 51, from which pipe58 leads to heating coil 60. From the coil 60 pipe 52 leads to glycerideinlet pipe 6.

Within the column i are located two separating and re-spraying stationsindicated generally as 64 and 65, and shown in greater detail in Figs.

-4 and 6. Each of these includes a collecting funnel 60 equipped with aspray head 61 at the bottom thereof and also with tangentially arrangednozzles 68, the funnels being secured to and supported by the wall ofthe column. There is also provided at each of the stations 64 and 05 apair of perforated plates 10, H secured to the column wall andsupportingtherebetween a porous filtering mass 12 which, when hydrogenation insidethe column is desired. performs not only a filtration but also ahydrogenating function, and for such hydrogenating function comprises asuitable hydrogenation catalyst, as for example nickel. For example,nickel wool may be employed in order to accomplish both an emulsionseparating and hydrogenating functions. At the top of the column thereare also preferably placed a pair of perforated plates I4, 16 supportedby the column wall and carrying therebetween a similar porous filteringmedium 18.

Referring to Fig. 2, the column I therein is constructed similarly tothe column shown in Fig. 1, having separating and/or hydrogenatingstations 64 and 65 and a porous filtering mass 16 adjacent the top ofthe column, an outlet 28 'for fatty acids and an inlet 9 for glyceride.to-

gether with a separating tank It equipped and connected to the column Ias shown in Fig. 1. At the left of Fig. 2 is shown a series ofhydrogenation columns. Column 00 contains a mass of hydrogenatingcatalyst in the form of nickel splinters. It is also equipped with a rod8| provided with a series of pleats 82 for the purpose of withdrawingthe nickel splinters from the column 80 after the catalyst is spent. Itwill of course be understood that the column will be provided withsuitable opening means at the bottom thereof to permit this. withdrawal,this means being not specifically shown.

In column 83 the catalyst, for example nickel splinters, is supportedtherein within an elongated perforated basket 84. The basket containingthe catalyst may be withdrawn from the column when the catalyst isspent. A suitable opening, not specifically shown; is provided to permitthis withdrawal. Column 85 may be equipped with a catalyst by meanssimilar to that shown in column 00 or column 89. Column 86 is aseparating column provided with gauges or inspection means 97, 80, toindicate the levels of the glyceride and hydrogen gas, respectively.From the column 06 pipe 9i leads to pump 92 driven by motor 93 anddischarging the hydrogenated glyceride through inlet pipe 6 into thecolumn I.

Referring to Fig. 3, the columns shown here are constructed and equippedas shown in Fig. 1, these columns being connected together in series andtherefore providing in effect a single column having a larger number ofseparation stations than shown in Fig. l. The column 95 is equipped withwater inlet pipe 2 and spray head 3 anda bottom outlet I00 connected topipe IOI which terminates in spray head 3a in column 96. C01- umn 98 hasan outlet I02 at the bottom thereof connected to pipe I 03 whichterminates in the spray head th at the top of column 9i. Column 91 hasan outlet I04 at the bottom thereof and it will be understood that thepipe 104 is connected to a separation tank It equipped as shown in Fig.l, and also connected to column 9? in the same manner that tank It isconnected to column I in Fig. 1. Glyceride inlet 0 terminating in sprayhead i is located at the bottom of column 91. From a point adjacent thetop of column 91 pipe I06 leads to column 90 and terminates in sprayhead Ia. at the bottom thereof, and in like manner from a point adjacentthe top of column 98 pipe I01 leads to column 95 and terminates in aspray head 'Ib at the bottom thereof. From the top of column 95 fattyacid outlet pipe 28 leads to a heat exchanger, and it will be understoodthat this will be constructed substantially as shown in Fig. 1. It willalso be understood that water and oil tanks, pumps and heating coilswill be arranged in substantially the same manner and for the samepurposes as shown in Fig. 1, to heat the glyceride and water,respectively, the heated water entering the column 05 through the pipe 2and the heated glyceride entering the column 91 through the inlet 6.Thus the columns 90, 96 and 91 are arranged for counter-current flow ofglyceride and water in substantially the same manner as that flow occursin the single column shown in Fig. 1.

Referring to Fig. 5, the columns I08, I09 and H0 are arranged for thecounter-current flow of glyceride and hydrogen prior to introductioninto a column I as shown in Fig. 2. The column I08 has a glyceride inletII2 provided with valve II3, adjacent the top thereof, and at the top ahydrogen outlet pipe Ilt provided with valve H5. From the bottom ofcolumn I09 pipe I ll leads to column I09, from the bottom of which pipeII8 leads to column IIO. Adjacent the bottom of column IIO outlet pipeI20 equipped with valve I2I is provided. At the top-of column IIO thereis provided an inspection gauge or glass I22 and Having described andillustrated apparatus in which the processes of the invention may becarried out, illustrative embodiments of those processes will now bedescribed.

water from the tank 4,4 and glyceride from the tank ID are passed bymeans of pumps 4| and 01, respectively, through heating coils l and 00,respectively, and are delivered to the column I (see Fig. 1) throughpipes 2 and I connected to sprays 3 and 1, respectively. For the sake ofsimplicity the glyceride will be referred to as oil. In the heatingcoils the water and oil are heated to a temperaturesufiicient tomaintain the water and oil in the column I at an oil splittingtemperature, the range of which will vary and in typical instances maybe between about 480 F. and 570 F. The pressure in the tower, maintainedtherein by means of valves 20 and I0, will be sufllcient to maintain thewater substantially in the liquid phase at these high temperatures, andthe flow of water and oil in the column I is counter-current.

In the zone of column I between the stations 85 and the spray I, anemulsion composed of a fatty component and a glycerine-water com ponentis formed. This emulsion, by contact withthe porous filtering mass I2,is separated into its fatty component and its glycerine-water component.The fatty component continues to pass upwardly and in so doing is forcedthrough the tangentially arranged nozzles which imparts to the fattycomponent a swirling motion serving to re-spray it into the descendingmass of water in the zone immediately above the separation station 65.The separated glycerine-water component is arrested by the porousfiltering mass I2 and is caused to pass downwardly from the station 65.At the same time water passing downwardly from the station 84 to thestation '05 is collected in the funnel and in its further downwardpassage is forced through the spray 81 and thereby re-sprayed into thezone below the sta-- tion 65. A similar process occurs at the station64. I It will therefore be apparent that at each separating andre-spraying station the upwardly moving emulsion is separated into itsfatty component and glycerine-water component. The fatty componentpasses upwardly from said station into the counter-currently descendingstream of water, whereas the separated glycerine water component insteadof passing upwardly is arrested and caused to pass downwardly. Ittherefore follows that upward movement of the separated glycerine-watercomponent into the successive zones is prevented in the concentration,and therefore the fat splitting activity of the water in each of saidzones is increased.

As many of the separating stations as desired may be provided either inthe same column, as shown in Fig. 1, or in a series of connectedcolumns, as shown in Fig. 3. The increase of fat splitting activity inthe several zones is such that with an apparatus as shown in'Fig. 1having three fat splitting zones it is possible to obtain at a pressureof about 300 pounds per square inch and a temperature of about 400 F.,an efllciency of splitting or hydrolysis of about 99 percent,particularly if a hydrolytic catalyst such as zinc oxide or caustic sodabe employed. The hydrolysis results in a solution of glycerine whichcollects in tank It and is removed therefrom through the pipe I8. Anyfatty material mixed with the glycerine solution will separate therefromin the tank It and return to the column through the pipe I6. From thetop of the column and after passing through the porous filtering mass I8at the top thereof, the fatty acid passes through the pipe 23 into theheat exchanger 21, the pressure therein being reduced to any .desiredextent which may, for example, be about 90 pounds per square inch, bymeans of pressure reducing valve 20. In the heat exchanger the pressureof the fatty acid is reduced, as also is its temperature, the coolingeffect being obtained by water passing into the heat exchanger throughthe pipe 4i and out of the exchanger through the pipe 42. The coolingwater is, of course, heated by heat exchange with the hot fatty acid andis led from the pipe 42 to the tank 44. Upon reducing the pressure ofthe fatty acid in the heat exchanger 21 and cooling it therein, anywater dissolved in the fatty acid under the high temperature andpressure existing in the column I separates out and is collected inseparating tank 30, from which the water is drawn off through pipe 00provided with valve 31. This water may be supplied to storage tank 44.The separated fatty acid is withdrawn from the tank 30 through pipe 38provided with valve 30.

In the event that it is desired to effect hydrogenatlon within thecolumn I, the porous filtering masses I2 and I0 will be selected so asto provide not only an emulsion separating function but also ahydrogenation function and may, for example, for this purpose becomposed of nickel wool or nickel splinters. Hydrogen is introduced intothe column I for hydrogenation purposes through the pipe I0 and excesshydrogen will then be vented from the heat exchanger by operation of thevalve 52 in the pipe 50.

The method of hydrolysis carried out in the apparatus shown in Fig. 3 isin general similar to themethod of hydrolysis carried out in theapparatus of Fig. 1. Heated water is sprayed downwardly into the column05 through the pipe 2 and spray 3 and heated oil is sprayed upwardly inthe column 91 through the pipe Ii and spray I. Glycerine solution isremoved from the column 95 throughpipes I00 and "II and is sprayeddownwardly in column 96 by spray 3a. In like manner glycerine solutionis removed from the bottom of column 96 through pipe I02, passes throughpipe I03 and is sprayeddownwardly in column 91 from the spray 3b. Thefinal and most concentrated glycerine solution is withdrawn from thebottom of column 91 through the pipe I04. The oil sprayed in the column96 upwardly from the column 9'! is converted into fatty acid bycountercurrent flow in contact with the hot water being carried from onecolumn to the other through the pipes I06 and I01, respectively, andbeing sprayed upwardly by the sprays Ia and lb located in columns 88 and95, respectively. The fatty acid product is withdrawn from the columnthrough the pipe 23. It will be noted that the apparatus of Fig. 3provides nine splitting zones. Of course, hydrogen may be introducedinto each of the columns 05, 98 and 81 for the same purpose and insubstantially the same manner as shown in the description of theapparatus in Fig. 1, and in this case the porous filtering masses I2 andI6 will be chosen so as to constitute not only porous filtering mediabut also hydrogenation catalysts.

Now referring to that phase of the invention which involvespre-hydrogenation of the glyceride prior to hydrolysis and immediatetransfer of the hydrogenated glyceride without cooling from thehydrogenation apparatus to the oil or fat splitting column, referencewill be had to Figs. 2 and 4 which respectively show methods forconcurrent and countercurrent ire-hydrogenation in conjunction with theimmediately following glyceride splitting step.

Referring to Fig. 2, oil and hydrogen enter the column 80 through inlets11 and I8, respectively,

it being understood that the oil will be heated to a hydrogenationtemperature. The oil and hydrogen pass upwardly in the column to, thatis,

concurrently in that column, and pass similarly in column 83 and column85, and the hydrogenated oil together with excess hydrogen pass into thedrawn from the bottom of the column 86 through the pipe 9i and pump 92and immediately discharged into the splittmg column i through the inlet3.

In the'pre-hydrogenation step the hydrogen and oil may flowcounter-currently, and for this purpose the apparatus shown in Fig. 5may be employed. In this apparatus oil flows into the column led throughthe pipe H2, then into the column "is through the pipe ill and then intothe column iiii through the pipe lit and finally out of the column lidthrough the pipe I20 and will then be immediately discharged into thefat splitting column i, as illustrated in Fig. 2. Hydrogen will beintroduced into the column iiii through the pipe 62% and will passthrough the respective columns counter-current to the oil, passing fromcolumn lid through the pipe i2! to the column Hi9, from the column W9through the pipe H28 to the column Hi8, and out of the column I08through the pipe H4. It will be understood that the columns shown inFig. 5 will be provided with hydrogenation catalytic means as, forexample, as illustrated in Fig. 2.

I claim:

1. In the process of continuous counter-curasiaeso the upward now ofsaid separated glycerinewater component and causing it to passdownwardly from said station; whereby a plurality of separate fatsplitting zones separated by said emulsion-separating stations aremaintained in said column, the upward movement of said separatedgiycerine-water into each of said zones is prevented and theconcentration and therefore the fat splitting activity of the water ineach of said zones is thereby increased; and continuously passing fat,including said separated fatty component, from a lower zone into thenext sue ceeding upper zone. v

t. In the process of continuous counter-current hydrolysis of iatwherein a body of fat flows upwardly in a column against a downwardlyflowing rain of water maintained under pressure in said column in theliquid phase at iat splitting temperatures and in which an emulsioncomposed of a fatty component and a glycerinewater component is formed;the improvement which comprises passing said emulsion in contact with aporous filtering medium and thereby separating said emulsion into itsfatty component and rent hydrolysis of fat wherein a body of fat flowsupwardly in a column against a downwardly flowing rain of watermaintained under pressure in said column in the liquid phase at fatsplitting temperatures and in which an emulsion composed of a fattycomponent and a glycerlnewater component is formed; the improvementwhich comprises passing said emulsionin contact with a porous filteringmedium and thereby separating said emulsion into its fatty component andits glycerine-water component at each of a plurality of stations in saidcolumn; arrestingthe upward flow of said separated glycerlnewatercomponent and causing it to pass downwardly from said station; whereby aplurality of separate fat splitting zones separated by saidemulsion-separating stations are maintained in said column, the upwardmovement of said separated glycerine-water into each of said zones isprevented and the concentrationv and therefore the fat splittingactivity of the water in each of said zones is thereby increased; andcontinuously passing fat, including said separated fatty component, froma lower zone into the next succeeding upper zone.

2. In the process of continuous counter-current hydrolysis of fatwherein a body of fat flows upwardly in a column against a downwardlyflowing rain of water maintained under pressure in said column in theliquid phase at fat splitting temperatures and in which an emulsioncomposed of a fatty component and'a glycerinewater component is formed;the improvement which comprises filtering said emulsion and itsglycerine-water component at each of a plurality of stations in saidcolumn; arresting the upward flow of said separated glycerine-watercomponent and causing it to pass downwardly from said station; whereby aplurality of separate fat splitting zones separated by saidemulsion-separating stations are maintained in said column, the upwardmovement of said separated glycerine-water into each of said zones isprevented and the concentration and therefore the fat splitting activityof the water in each of said zones is thereby increased; continuouslypass-,

ing fat, including said separated fatty component, from a lower zoneinto the next succeeding upper zone and mixing it with water in saidupper zone by imparting a swirling movement to said fat, and collectingglycerine-water at each of said stations and spraying it downwardly intothe ascending fat.

4. In the'process of continuous counter-current hydrolysis of fatwherein a body of fat capable of hydrogenation flows upwardly in acolumn against a downwardly flowing rain of water maintained underpressure in said column in the liquid phase at fat splittingtemperatures and in which an emulsion composed of a fatty'component anda glycerine-water component is formed; the improvement which comprisespassing said emulsion in contact with a porous filtering mediumcomprising a nickel hydrogenation catalyst and thereby separating saidemulsion into its fatty component and its glycerinewater component, ateach of a plurality of stations in said column; arresting the upwardflow of said separated glycerine-water component and thereby separatingit into its fatty component 1 causing it to pass downwardly from saidstation; whereby a plurality of separate fat splitting zones separatedby said emulsion-separating stations are maintained in said column, theupward movement of said separated glycerine-water into each of saidzonesis prevented and the concentration and therefore the fat splittingactivity of the water in each of said zones is thereby increased;continuously passing fat, including said separated fatty component, froma lower zone into the next succeeding upper zone through said filteringmedium; introducing hydrogen into said column and effectinghydrogenation of fat at each of said stations in addition to the abovementioned separation of fat from said emulsion.

BARUCH WINER.

